Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Testing and Assessment of coatings in the field Advanced Training Course (ATC3) Biofouling & Bioadhesion Processes Dr David Williams, International Paint Ltd Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Presentation Content • Introduction • Why is field testing important? • Laboratory vs. field • Static immersion testing • Panel design & location • Assessment Methods • Analysis • Biofouling adhesion measurements • Dynamic field trials & test patches Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. The Development Cycle Laboratory Tests/Assays Test-patching Field Trials Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. What do we want to measure? • Antifouling (deterrence) performance • Longevity (> 5years) • Variation in performance • Foul release performance • Multiple fouling types • Coating adhesion • Over-coating over primer and self • Blistering or degradation • Physical changes • Loss of mechanical integrity • UV degradation at waterline • Polishing/erosion rate • Colour Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Laboratory vs. Field testing Factor Laboratory Field Fouling Challenge Known, single species Multiple species, uncontrolled Temperature, salinity & pH Known & measured Uncontrolled, monitored? Flow Static or characterised (flow cell) Uncontrolled (tidal?) Light exposure Controlled Uncontrolled Immersion/ test period Relatively short (hours, days, weeks) Can be long (>5 years!) Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Minimising variation • Immersion of painted panels on rafts • Static test (accelerated) • Relative test Factors that affect fouling: Test conditions cannot be reproduced: • Must make comparisons relative to a standard • Trials must be planned to minimise variation due to these factors Variation Raft Design light exposure water flow flotsam / jetsam accumulation grazing species Assessment consistency frequency accuracy categories / rating system colour thickness Paint batch variation age surface characteristics Environmental Conditions seasonality pH, temperature, salinity tidal flow / range FW influx fouling challenge (flora and fauna)pollution geographic location Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Antifouling coating testing Purpose: To predict which coatings would give best in-service antifouling performance on a real vessel NOT To provide an absolute census of marine biology resident on the panel! Ideal Test: • Immerse panels under exactly the same conditions • Same time • Same location • Obtain a direct comparison between coatings Reality: • Need to compromise! • Immerse adjacent panels at the same time • Not a direct comparison between coatings Sources of Uncertainty: Assessment Error Assessment Error Variation in fouling pressure + Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Test method selection There are a major considerations when selecting a test method/design • What are you trying to find out? • Panel design • No replicates, • Size and type of substrate • Location • Immersion site(s) • Depth of panel • Assessment regime • Data quality vs. Resource D ata Q uality Resource Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Panel Design Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Variation in fouling pressure Is this significant for a 2’x2’ panel? Slime / Fish Effects Hydroid / Weed Variation Weed Variation All coatings are the same Hard Bodied Animal Variation Zonation and stratification of fouling settlement results in a non-uniform fouling challenge Fouling variation Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Antifouling Raft Testing Historical Raft Testing using coating strips 50 60 70 80 90 100 K701 K702 K703 K704 K705 K706 K707 K708 K709 A F IM M R a ti n g Which is the best coating? - They’re all the same(!) • Fouling is unpredictable. Fouling challenge can vary significantly even over the area of a 2‟ x 2‟ panel • Sensitivity of this test is low • Limit of data quality available is low Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Non-biocidal Surfaces • In non-biocidal systems different organisms respond differently to the different coating surfaces • Harder to determine true performance • Strip testing does not lend itself to statistical analysis of data • Subtleties of performance differences can be missed 1 1 1 2 2 2 3 3 3 Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Variation in fouling pressure How can we minimise the effect this has on our testing? This has been thought about before… Rearrange Unequal distribution of fouling challenge More equal distribution of fouling challenge 6X6 layout will provide: • Fairer test of coatings • Better quality data Minimsing variation Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. 1 2 3 4 ST CT ST CT 1 2 3 4 3 4 ST CT 1 2 CT 1 2 3 4 ST 4 ST CT 1 2 3 2 3 4 ST CT 1 Panel standard design • 10x10cm squares • Natural variance in fouling is accounted for • Each coating appears in each row and each column (Latin Square variant) • Coatings are tested next to a standard and a control • Standard (A/F product) • Control (Primer) • Panel edged and backed with a non-biocidal coating Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Raft 4 Raft 5 Intersite variation • Immersion at multiple test-sites provides information about variation of performance with • Fouling challenge (tropical vs. temperate) • Other environmental factors – temperature, salinity, flow etc. Viareggio, Italy Changi, Singapore Newton Ferrers, UK Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Assessment Methods • Better data = more sensitive analyses • Measurements • Percent cover • Number of individuals • Size of individuals • Biomass • Species • Percent cover • Visual • Stereology • Image analysis Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Percent Cover Measurements • Visual Assessment • Quickest and cheapest • Widely used in field ecology • Stereology • Robust statistical approach • Widely used in medicine • Can be use in field with overlay or gridded quadrats • Commonly used with digital photographs • Image analysis • Hard to segment biofouling images • Need manual tracing and filling • Slow, very slow Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Comparison of methods • Meese & Tomich (1992) • Compared visual, stereology, and manual digital segmentation • Visual and stereology not good for rare (<1%) species, otherwise robust • Visual estimation recommended for field work • Vanha-Majamaa et al (2000) • Compared visual and automatic and manual segmentation • Number of species detected higher visually • Visual estimation faster and as precise as manual segmentation • Drummond & Connell (2005) • Compared in field visual estimation vs lab stereology (random/square arrays, different densities of dots), and manual digital segmentation. • Precision unaffected by density or environment. • Major concern number of replicates and area analysed therefore swiftest (visual) often preferred Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. 10% 10% Visual Assessment – Scattered vs. Local Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. What to measure • Species level • Tedious • Requires high level taxonomic skills • Makes inter-site comparisons difficult • Functional group • Categorising organisms by niche • Less taxonomy but more ecological knowledge needed • Very useful for understanding function of communities • Fouling Category • Hard, soft, weed, micro • Blurs data but maps nicely onto hydrodynamic studies • Quick, requires little taxonomy • Longitudinal and spatial comparisons easy A ssessm ent S peed D at a C om pl ex ity Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Assessment Methods Barnacles (Cthalamus stellatus) Weed (Enteromorpha intestinalis) Hydroids (Tubularia indivisa) Microalgae Red Brown Green Macroalgae Unlimited Limited Soft Bodied Barnacles Tube Worms Mussels Other Hard Shelled Animal Fouling Organism Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Organisms on Panels at UK test Sites Organism Category Burnham Ferrers Anemone Soft Barnacle Hard Bryozoan bushy Hard Bryozoan flat Hard Hydroid Soft Mud Shrimp - Mussel Hard Oyster Hard Slime Micro Slipper limpet - Sponge Soft Tube worm Hard Tunicate Clear/orange Soft Tunicate Colonial Soft Tunicate Leathery Soft Weed brown Weed Weed green Weed Weed red Weed Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Soft Hard Micro Weed Visual Assessment Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Image Analysis • Remote assessments using Image Analysis • Reduces raft time • Increases confidence in data(?) • Less assessment is required (only relevant panels) • Assessment can be carried out at any time (and repeated) • Issues • Need high quality photos – Ideally one photo (>12 MP) • Need to train people in taking of photographs • Storage of photos • Resource is required to carry out analysis at desktop Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Image Analysis – % Cover Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. • Stereology interface with user controls for zooming, panel tracking and results export to Excel • Adds data to a standard worksheet • Permits assessment of multiple panels on single photograph of same board Image Analysis – Stereology • Freeware from NIH • Java based • 80,000 users, platform independent • Easy to implement personal routines and interface Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Panel number 408F Micro(%) : 8 Soft(%) : 25 11 %C.I : 95 Weed(%) : 10 Hard(%) : 40 Mean normalised % CI Mean normalised % CI worse better 1620 6.33 -67.00 7.48 253.33 -2350.00 299.33 better 0 1 1602 69.17 -4.17 13.49 2766.67 163.33 539.53 - 0 0 1608 94.83 21.50 3.14 3788.33 1185.00 131.62 - 0 0 1614 90.67 17.33 10.05 3576.67 973.33 385.73 - 0 0 ST 73.33 0.00 18.54 2603.33 0.00 1119.04 - - - CT 96.67 23.33 6.53 3866.67 1263.33 261.33 - 0 0 0 0 Coating 1620 1602 1608 1614 ST CT Total 1620 - 0 0 0 0 0 0 1602 1 - 0 0 0 0 1 1608 1 1 - 0 0 0 2 1614 1 0 0 - 0 0 1 ST 1 0 0 0 - 0 1 CT 1 1 0 0 0 - 2 HIGHEST SCORE IS THE WORST Is Vertical coating better than Horizontal coating? 3rd 2nd 2nd 3rd 2nd Coating details 0 Better than Std? % Penalties : Ranking based on H. rating Best No. weeks immersed 0 Fouling % Hydrodynamic rating 0 0 0 0 Total fouling coverage (%) per coating 0 10 20 30 40 50 60 70 80 90 100 1620 1602 1608 1614 ST CT F o u lin g c o ve ra g e (% ) 95 Total hydrodynamic rating per coating 0 500 1000 1500 2000 2500 3000 3500 4000 1620 1602 1608 1614 ST CT H yd ro d yn am ic r at in g 95 Fouling coverage (%) by fouling category 0 10 20 30 40 50 60 70 80 90 100 1620 1602 1608 1614 ST CT F o u lin g c o ve ra g e (% ) Micro Weed Soft Hard 95 Hydrodynamic rating due to fouling 0 500 1000 1500 200 2500 3000 3500 4000 1620 1602 1608 1614 ST CT H yd ro d yn am ic r at in g Micro Weed Soft Hard 95% Conf.% Conf. % Conf.% Conf. Panel number 408F Micro(%) : 8 Soft(%) : 25 11 %C.I : 95 Weed(%) : 10 Hard(%) : 40 Mean normalised % CI Mean normalised % CI worse better 1620 10.54 -58.84 10.60 421.77 -2223.13 424.15 better 0 1 1602 72.11 2.72 6.08 2884.35 239.46 243.23 - 0 0 1608 96.26 26.87 4.89 3785.03 1140.14 311.39 - 0 0 1614 90.82 21.43 10.97 3589.12 944.22 424.96 - 0 0 ST 69.39 0.00 22.98 2644.90 0.00 1044.28 - - - CT 100.00 30.61 0.00 4000.00 1355.10 0.00 worse 1 0 1 0 Coating 1620 1602 1608 1614 ST CT Total 1620 - 0 0 0 0 0 0 1602 1 - 0 0 0 0 1 1608 1 1 - 0 0 0 2 1614 1 1 0 - 0 0 2 ST 1 0 0 0 - 0 1 CT 1 1 0 0 1 - 3 HIGHEST SCORE IS THE WORST Is Vertical coating better than Horizontal coating? 3rd 3rd 2nd 4th 2nd Coating details 0 Better than Std? % Penalties : Ranking based on H. rating Best No. weeks immersed 0 Fouling % Hydrodynamic rating 0 0 0 0 Total fouling coverage (%) per coating 0 10 20 30 40 50 60 70 80 90 100 1620 1602 1608 1614 ST CT F o u lin g c o ve ra g e (% ) 95 Total hydrodynamic rating per coating 0 500 1000 1500 2000 2500 3000 3500 4000 1620 1602 1608 1614 ST CT H yd ro d yn am ic r at in g 95 Fouling coverage (%) by fouling category 0 10 20 30 40 50 60 70 80 90 100 1620 1602 1608 1614 ST CT F o u lin g c o ve ra g e (% ) Micro Weed Soft Hard 95 Hydrodynamic rating due to fouling 0 500 1000 1500 200 2500 3000 3500 4000 1620 1602 1608 1614 ST CT H yd ro d yn am ic r at in g Micro Weed Soft Hard 95% Conf.% Conf. % Conf.% Conf. In-field Assessment Image Analysis Assessment Image Analysis – In-field vs. Desk-top Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. How to analyse? • Total percent cover • Percent cover by type • Hydrodynamic effect • Multivariate and univariate analyses • ANOVA, MANOVA, GLZM, GEE Hydrodynamic Rating vs. Time 0 10 20 30 40 50 60 70 80 90 100 0 5 10 15 20 25 30 35 40 Time (weeks) H . R at in g 2325 2326 2327 2328 ST CT Error Bars = 95% Conf. Intervals Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Performance Assessment Phoenix Anti-Fouling Immersion Test Data Panel 66-34F 1st Assessment Phoenix Panel Number: 34F Immersion Date: 17-Nov-99 Immersion Site: Raft Panel Bay Number: AH7F Assessment Date: 06-Jan-00 Country : Trial Row Column Coating % Microfouling % Weed % Soft-Bodied Animal % Hard-Bodied Animal % Total Fouling A1 1 1 215 0 20 70 5 95 A2 1 2 216 0 5 85 0 90 A3 1 3 217 0 70 5 0 75 A4 1 4 218 0 20 70 0 90 A5 1 5 ST 0 10 45 5 60 A6 1 6 CT 0 0 95 5 100 B1 2 1 ST 0 10 75 15 100 B2 2 2 CT 0 5 75 10 90 B3 2 3 215 0 20 55 0 75 B4 2 4 216 0 65 10 0 75 B5 2 5 217 0 15 10 0 25 B6 2 6 218 0 5 90 5 100 C1 3 1 217 0 0 60 0 60 C2 3 2 218 0 0 70 5 75 C3 3 3 ST 0 10 50 15 75 C4 3 4 CT 0 0 90 10 100 C5 3 5 215 0 0 90 5 95 C6 3 6 216 0 5 55 0 60 D1 4 1 CT 0 5 70 20 95 D2 4 2 215 0 0 50 30 80 D3 4 3 216 0 0 55 5 60 D4 4 4 217 0 0 30 0 30 D5 4 5 218 0 0 85 10 95 D6 4 6 ST 0 5 85 0 90 E1 5 1 218 0 10 20 30 60 E2 5 2 ST 0 5 45 30 80 E3 5 3 CT 0 0 60 40 100 E4 5 4 215 0 0 65 15 80 E5 5 5 216 0 0 55 5 60 E6 5 6 217 0 10 40 0 50 Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Data Analysis Plot of Mean% Fouling of Coatings by Fouling Category Assessment 1 0.00 20.00 40.00 60.00 80.00 100.00 A B C D ST CT Coating M ea n % F ou lin g C ov er Microfouling Weed Soft-Bodied Animal Hard-Bodied Animal Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Significance Testing NORMAL DATA • Analysis of Variance (ANOVA) is used to determine whether there are any significant differences • A test of comparisons (Dunnett,Tukey, Bonferroni) can be used to determine which coatings are significantly different from each other NON-NORMAL DATA • Non-parametric analysis is ANOVA carried out (Kruskal-Wallis) • Coatings are mean ranked 0 1 0 2 4 6 8 10 12 14 16 Fr e q u e n cy Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Statistical Methods - ANOVA Coating Comparisons Test 1-way between subjects ANOVA Hard-Bodied by Coating: A, B, C, Control, D, Standard Performed by dwilliams Date 24 October 2002 n 36 Hard-Bodied by Coating n Mean SD SE A 6 0.304 0.199 0.0813 B 6 0.141 0.167 0.0683 C 6 0.038 0.092 0.0376 Control 6 0.450 0.197 0.0803 D 6 0.263 0.188 0.0768 Standard 6 0.333 0.198 0.0808 Source of variation SSq DF MSq F p Coating 0.641 5 0.128 4.06 0.0062 Within cells 0.947 30 0.032 Total 1.589 35 Bonferroni Contrast Difference 95% CI A v Standard -0.029 -0.311 to 0.253 B v Standard -0.192 -0.474 to 0.091 C v Standard -0.295 -0.578 to -0.013 (significant) Control v Standard 0.117 -0.165 to 0.399 D v Standard -0.070 -0.352 to 0.212 Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Hydrodynamic Rating to Measure Static Antifouling Performance. Fouling Coverage; 37 weeks; Changi 0 10 20 30 40 50 60 70 80 90 100 2325 2326 2327 2328 ST CT F o u lin g c o ve ra g e (% ) Error Bars = 95% Conf. Intervals Micro Weed Soft Hard Step 1: Assessment of fouling coverage from antifouling board (6x6 Latin square design). Fouling coverage broken down into four categories. Hydrodynamic Rating; 37 weeks; Changi 0 10 20 30 40 50 60 70 80 90 100 2325 2326 2327 2328 ST CT H yd ro d yn am ic R at in g Error Bars = 95% Conf. Intervals Hydrodynamic Factors: Micro: 8 Soft: 25 Weed: 10 Hard: 40 Step 2: Cumulative H- rating determined by accounting for impact on vessel hydrodynamics of each fouling type (M.P. Schultz (US Navy), Biofouling 2007) Time Weighted Average Hydrodynamic Rating 0 10 20 30 40 50 60 70 80 90 100 0 5 10 15 20 25 30 35 40 Time (weeks) T im e W td . A ve ra g e H . R at in g 2325 2326 2327 2328 ST CT Step 3: Frequent, regular assessments allow for performance monitoring against time. Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Biofouling Adhesion Measurements • Various methods used from simple to complex • Standard brush test • Barnacle Adhesion Measurements • Water-jet testing • Hydrodynamic Foil Measurements • Can measurements be used to predict required vessel speed for release? Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Barnacle Adhesion Measurement • Commonly used Barnacle adhesion strength in shear (push-off) ASTM D5618-94 • Applying a force, normally with a hand-held force gauge, parallel to the attached plane of the barnacle at an approximate rate (4.5Ns-1) until it is removed from the surface • Measuring the attachment area, either by measuring the diameter of the barnacle or using a flat-bed scanner and image analysis to directly determine the area Automated In-field Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Barnacle Adhesion Strength – In-field Data • Issues • Species to species variation • Growth on defects • Growing enough barnacles! Foul-Release - In-field data barnacle push-offs 0 5 10 15 20 25 30 35 40 45 A B C D IN TE RS LE EK SI LC IO NE A CO NT RO L Coating Type A dh es io n Fo rc e (P S I) A B C Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Water-jet Testing • Water-jet Variable pressure • Fouling type versus pressure • Comparative test Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Dynamic Test Methods • Must be representative of ship‟s hull hydrodynamics • Flow characteristics should be well characterised - eq. ship speed • Must give reproducible and reliable results Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Drum Rotors • Drum diameter and rotation rate selected to give desired speed • „Pseudo-test patch‟ • Ideal for antifouling, polishing rate and foul release testing • Power must be supplied to raft • ASTM D 4939 – Static / Dynamic Exposure • Alternates between static and dynamic exposure to simulate in- service conditions • Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Other Dynamic Tests Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Instrumented foil • Test developed by Professor Geoff Swain at FIT • Foil mounted in rear of powerboat • Specially designed window allows exact fit of panel below boat • Panel removed, photographed, cleaned and re-run for clean panel comparison data Foul-release coating after 1minutes @20 knots Foul-release coating after cleaning Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Intersleek Testing After 4 knots for 1 min After 7.5 knots for 1 min After 12 knots for 1 min After 16.5 knots for 1 min After 20 knots for 1 min Before Testing Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Test-patches • The ultimate antifouling and in-service performance test • Suitable for all end-uses • Ships, yachts, aquaculture etc. • Vary is size small (1m2) to large (100m2) Benefits • “Real-life” performance • Dynamic and static • Demonstrate performance to customer Concerns • Expensive • Application/dry-dock costs • Assessment costs • Number of patches? • Risk – failure can be expensive! Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Test Patches – Types • Conventional Application • Yachts - Brush/roller • Marine vessels - Airless spray • Aquaculture – dipping • Magnetic/Adhesive Panels/Tape applied to vessels in dry dock • Inspection by diver/drydock to retrieve panel/tape Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Test-patch assessment Yachts • Hauled and assessed visually or by image analysis Ships • Ideally assessed in dry-dock • Underwater inspections • Good water conditions • Correct equipment & training Marine CoatingsFor internal use only – not to be circulated to customers or outside International Paint Ltd. Answers & Questions! Picture Hard Soft Weed Micro Total 1 62 4 0 21 87